CN106241761B - A kind of processing method of useless concentrated phosphoric acid - Google Patents
A kind of processing method of useless concentrated phosphoric acid Download PDFInfo
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- CN106241761B CN106241761B CN201610598816.8A CN201610598816A CN106241761B CN 106241761 B CN106241761 B CN 106241761B CN 201610598816 A CN201610598816 A CN 201610598816A CN 106241761 B CN106241761 B CN 106241761B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
- C01B25/2372—Anionic impurities, e.g. silica or boron compounds
- C01B25/2377—Sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of processing methods of useless concentrated phosphoric acid, belong to multipurpose use of the three wastes technical field.This method comprises the following steps：Adjust sour, thick desulfurization, thick desulfurization press filtration, fine de-sulfur, fine de-sulfur press filtration and filter residue mixing；The processing method of useless concentrated phosphoric acid provided by the invention; using the technological process for adjusting sour, thick desulfurization, thick desulfurization press filtration, fine de-sulfur, fine de-sulfur press filtration and filter residue mixing; the useless concentrated phosphoric acid generated in every profession and trade production process can be handled; obtain fertilizer grade phosphoric acid and commercial sulphuric acid salt; turn waste into wealth while resource is saved; both natural ecological environment is protected, while adds benefit；This method is simple for process, easy to operate, at low cost, is suitble to industrialized production.
Description
Technical field
The present invention relates to a kind of processing methods of chemical waste, and in particular to a kind of processing method of useless concentrated phosphoric acid belongs to
Multipurpose use of the three wastes technical field.
Background technology
Phosphoric acid is a kind of relatively common acid, is used primarily in the manufacture of phosphate fertilizer；Also often make in the chemical polishing of metal
Use phosphoric acid；In addition in the nitrification of aromatic compound using phosphoric acid can play the role of adjust adjacency pair than, using after a period of time by
In the catalytic action that can influence to polish or nitrify of increasing of impurity, spent acid is formd, the complicated component of the spent acid is unfavorable for recycling
It utilizes, in general pure waste phosphoric acid can have good recycling on chemical fertilizer, also there is the method for comparative maturity at present, main
To be exactly to be used for producing the products such as ammonium phosphate, calcium phosphate or calcium monohydrogen phosphate, as the Chinese patent of Patent No. CN101274754 carries
A kind of method using waste ammonia liquor and waste phosphoric acid production ammonium phosphate is gone out, this method utilizes the waste ammonia liquor containing ammonia more than 7%, strong
Heating distillation is carried out under the action of oxidation catalyst, by waste phosphoric acid neutralization reaction of the ammonia of distillation directly with 25~92%, then
It dries.Chinese patent such as Patent No. CN103738933A disclose recycled in a kind of waste phosphoric acid from sulfur acid it is high-purity
The method of calcium monohydrogen phosphate is spent, this method adds in active powdered carbon, filters and adds in excessive calcium carbonate suspension or calcium hydroxide breast
Calcium sulphate dihydrate and aluminum phosphate is obtained by filtration in liquid, while with calcium carbonate suspension and calcium hydroxide emulsion in obtained filtrate
Form add in the calcium of theoretical amount needed for phosphoric acid, then plus pure water filtration drying obtains the dicalcium phosphate dihydrate of high-purity, beats
It starches, separation of solid and liquid, is dried to obtain the calcium phosphate dibasic anhydrous of high-purity.The invention reduces the phosphorus-containing wastewater of discharge highly acid to ring
The phosphatic raw materials that the phosphorus in waste phosphoric acid solution only has use value are recycled in the harm in border.
A kind of phosphate discharge liquid is disclosed for the Chinese patent of the processing such as Patent No. CN104973581A of phosphate discharge liquid
Processing method, this method handles phosphate discharge liquid using micro-filtration, anion exchange, cation exchange, membrane distillation successively,
Recycle phosphoric acid therein.But the invention is swapped in processes using zwitterion column, and it is of high cost, it produces in process of production
Raw substantial amounts of waste liquid, waste of resource are unfavorable for industrialization large-scale production.
The content of the invention
The shortcomings that it is an object of the invention to overcome the prior art, provides a kind of processing method of useless concentrated phosphoric acid.
The purpose of the present invention is achieved through the following technical solutions：A kind of processing method of useless concentrated phosphoric acid, it includes following
Step：
S1. acid is adjusted：Useless phosphoric acid,diluted is added in useless concentrated phosphoric acid to carry out adjusting acid, adjust the concentration of the waste phosphoric acid after acid for 16~
20%；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in thick desulfurizing agent and carry out thick desulfurization
Solidliquid mixture is obtained, it is 50~60 DEG C to control thick desulphurization reaction material temperature in kettle；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is sulfate precipitation, and the moisture content of the sulfate precipitation is 35~45%；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in desulfurizing agent and obtains secondary solid-liquid and mix
Object is closed, it is 50~60 DEG C to control fine de-sulfur material in reactor temperature；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is sulfate precipitation to obtain solid-state, and filtrate is product phosphoric acid；
S6. filter residue mixes：Sulfate precipitation obtained by sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Further, the mass percentage concentration for concentrated phosphoric acid of giving up described in step S1 is 60~70%, the useless phosphoric acid,diluted
Mass percentage concentration is 5~10%, and the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 3~5:1.
Further, thick desulfurizing agent described in step S2 is CaCO3, dosage be thick desulphurization reaction kettle in cannot generate it is heavy
It forms sediment.
Further, desulfurizing agent described in step S4 is BaCO3, dosage for filtrate weight obtained by step S3 4%~
6%.
Further, thick desulfurization filter press pressure described in step S3 is 0.6~1.0MPa, and filter cloth aperture is 300~350
Mesh.
Further, fine de-sulfur filter press pressure described in step S5 is 0.6~1.0MPa, and filter cloth aperture is 300~350
Mesh.
In the present invention：
In thick desulfurized step, manually by packed solid-state desulfurizer powder (CaCO3) unpack, using feeding intake, grapple is sent
It to thick desulphurization reaction kettle charge door, and pours into wherein, charge door sets dust gas gathering mask.
Due to SO4 2-With CaCO3Reactivity is higher than and PO4 3-、HPO4 2-、H2PO4 -Deng reactivity, i.e. CaCO3First with
SO4 2Reaction production sulfate hemihydrate calcium precipitate.The spent acid of every batch of is handled, SO in equal sample survey4 2-Content adds accordingly
CaCO3, by CaCO3Dosage control, with this prevent thick desulfurization workshop section generation synthos precipitation.
Reaction equation is as follows：
CaCO3+SO4 2-+2H+=CaSO4·1/2H2O↓+CO2↑+1/2H2O
The reactor off-gas of generation is carbon dioxide, which is exothermic reaction, and material in reactor temperature is about 50~60
DEG C, no more than acid decomposed by phosphoric acid temperature (480 DEG C), P will not be generated2O5, and phosphoric acid will not generate for low volatility acid reaction temperatures
Water vapour (100 DEG C), therefore the reactor off-gas is carbon dioxide, not phosphoric acid.
In fine de-sulfur step, solid-state desulfurizer powder (BaCO is put into fine de-sulfur reaction kettle3), further removal is useless
Sulfate radical in phosphoric acid.Reaction equation is as follows：
BaCO3+SO4 2-+2H+=BaSO4↓+CO2↑+H2O
The reactor off-gas of generation is carbon dioxide, which is exothermic reaction, and material in reactor temperature is about 50~60
DEG C, no more than acid decomposed by phosphoric acid temperature, and phosphoric acid is that low volatility is calculated, and reaction temperature will not generate water vapour, therefore the reactor off-gas
For carbon dioxide, not phosphoric acid.
The present invention has the following advantages：The processing method of useless concentrated phosphoric acid provided by the invention, using adjusting acid+thick desulfurization+thick
The technological process of desulfurization press filtration+fine de-sulfur+fine de-sulfur press filtration+filter residue mixing, can handle what is generated in every profession and trade production process
Useless concentrated phosphoric acid, obtains fertilizer grade phosphoric acid and commercial sulphuric acid salt, turns waste into wealth while resource is saved, both nature was protected to give birth to
State environment, while add benefit；This method is simple for process, easy to operate, at low cost, is suitble to industrialized production.
Specific embodiment
With reference to embodiment, the present invention will be further described, and protection scope of the present invention is not limited to following institute
It states.
Embodiment 1：A kind of processing method of useless concentrated phosphoric acid, it comprises the following steps：
S1. acid is adjusted：Dilute phosphorus that gives up that mass percentage concentration is 5% is added in the useless concentrated phosphoric acid that mass percentage concentration is 60%
Acid carries out adjusting acid, until the concentration for adjusting the waste phosphoric acid after acid is 16%, the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 3:1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in CaCO3Thick desulfurization is carried out to obtain
To solidliquid mixture, CaCO3Dosage is that cannot generate precipitation in thick desulphurization reaction kettle, controls material temperature in thick desulphurization reaction kettle
It spends for 50 DEG C；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is calcium sulfate precipitation, and the moisture content of the calcium sulfate precipitation is 35%, and the thick desulfurization filter press pressure is
0.6MPa, filter cloth aperture are 300 mesh；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in BaCO3Secondary solid-liquid is obtained to mix
Object is closed, it is 50 DEG C to control fine de-sulfur material in reactor temperature, the BaCO3Dosage be filtrate weight obtained by step S3
4%；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is barium sulfate precipitate to obtain solid-state, and filtrate is product phosphoric acid, and the fine de-sulfur filter press pressure is 0.6MPa, and filter cloth aperture is
300 mesh；
S6. filter residue mixes：Barium sulfate precipitate obtained by calcium sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Embodiment 2：A kind of processing method of useless concentrated phosphoric acid, it comprises the following steps：
S1. acid is adjusted：Added in the useless concentrated phosphoric acid that mass percentage concentration is 70% mass percentage concentration be 10% it is useless dilute
Phosphoric acid carries out adjusting acid, until the concentration for adjusting the waste phosphoric acid after acid is 20%, the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 5:
1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in CaCO3Thick desulfurization is carried out to obtain
To solidliquid mixture, CaCO3Dosage is that cannot generate precipitation in thick desulphurization reaction kettle, controls material temperature in thick desulphurization reaction kettle
It spends for 60 DEG C；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is calcium sulfate precipitation, and the moisture content of the calcium sulfate precipitation is 45%, and the thick desulfurization filter press pressure is
1.0MPa, filter cloth aperture are 350 mesh；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in BaCO3Secondary solid-liquid is obtained to mix
Object is closed, it is 60 DEG C to control fine de-sulfur material in reactor temperature, the BaCO3Dosage be filtrate weight obtained by step S3
6%；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is barium sulfate precipitate to obtain solid-state, and filtrate is product phosphoric acid, and the fine de-sulfur filter press pressure is 1.0MPa, and filter cloth aperture is
350 mesh；
S6. filter residue mixes：Barium sulfate precipitate obtained by calcium sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Embodiment 3：A kind of processing method of useless concentrated phosphoric acid, it comprises the following steps：
S1. acid is adjusted：Dilute phosphorus that gives up that mass percentage concentration is 8% is added in the useless concentrated phosphoric acid that mass percentage concentration is 65%
Acid carries out adjusting acid, until the concentration for adjusting the waste phosphoric acid after acid is 18%, the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 4:1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in CaCO3Thick desulfurization is carried out to obtain
To solidliquid mixture, CaCO3Dosage is that cannot generate precipitation in thick desulphurization reaction kettle, controls material temperature in thick desulphurization reaction kettle
It spends for 55 DEG C；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is calcium sulfate precipitation, and the moisture content of the calcium sulfate precipitation is 40%, and the thick desulfurization filter press pressure is
0.8MPa, filter cloth aperture are 320 mesh；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in BaCO3Secondary solid-liquid is obtained to mix
Object is closed, it is 55 DEG C to control fine de-sulfur material in reactor temperature, the BaCO3Dosage be filtrate weight obtained by step S3
5%；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is barium sulfate precipitate to obtain solid-state, and filtrate is product phosphoric acid, and the fine de-sulfur filter press pressure is 0.8MPa, and filter cloth aperture is
320 mesh；
S6. filter residue mixes：Barium sulfate precipitate obtained by calcium sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Embodiment 4：A kind of processing method of useless concentrated phosphoric acid, it comprises the following steps：
S1. acid is adjusted：Dilute phosphorus that gives up that mass percentage concentration is 6% is added in the useless concentrated phosphoric acid that mass percentage concentration is 68%
Acid carries out adjusting acid, until the concentration for adjusting the waste phosphoric acid after acid is 17%, the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 3:1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in CaCO3Thick desulfurization is carried out to obtain
To solidliquid mixture, CaCO3Dosage is that cannot generate precipitation in thick desulphurization reaction kettle, controls material temperature in thick desulphurization reaction kettle
It spends for 59 DEG C；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is calcium sulfate precipitation, and the moisture content of the calcium sulfate precipitation is 42%, and the thick desulfurization filter press pressure is
0.9MPa, filter cloth aperture are 330 mesh；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in BaCO3Secondary solid-liquid is obtained to mix
Object is closed, it is 53 DEG C to control fine de-sulfur material in reactor temperature, the BaCO3Dosage be filtrate weight obtained by step S3
4.5%；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is barium sulfate precipitate to obtain solid-state, and filtrate is product phosphoric acid, and the fine de-sulfur filter press pressure is 0.9MPa, and filter cloth aperture is
330 mesh；
S6. filter residue mixes：Barium sulfate precipitate obtained by calcium sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Embodiment 5：A kind of processing method of useless concentrated phosphoric acid, it comprises the following steps：
S1. acid is adjusted：Dilute phosphorus that gives up that mass percentage concentration is 9% is added in the useless concentrated phosphoric acid that mass percentage concentration is 62%
Acid carries out adjusting acid, until the concentration for adjusting the waste phosphoric acid after acid is 19%, the volume ratio of the useless concentrated phosphoric acid and useless phosphoric acid,diluted is 5:1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in CaCO3Thick desulfurization is carried out to obtain
To solidliquid mixture, CaCO3Dosage is that cannot generate precipitation in thick desulphurization reaction kettle, controls material temperature in thick desulphurization reaction kettle
It spends for 57 DEG C；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 is sent into thick desulfurization filter press and carries out press filtration, filtrate is standby
With obtained solid is calcium sulfate precipitation, and the moisture content of the calcium sulfate precipitation is 38%, and the thick desulfurization filter press pressure is
0.7MPa, filter cloth aperture are 310 mesh；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in BaCO3Secondary solid-liquid is obtained to mix
Object is closed, it is 51 DEG C to control fine de-sulfur material in reactor temperature, the BaCO3Dosage be filtrate weight obtained by step S3
5.5%；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, institute
It is barium sulfate precipitate to obtain solid-state, and filtrate is product phosphoric acid, and the fine de-sulfur filter press pressure is 0.7MPa, and filter cloth aperture is
310 mesh；
S6. filter residue mixes：Barium sulfate precipitate obtained by calcium sulfate precipitation obtained by step S3 and step S5 is mixed, is product
Sulfate.
Claims (3)
1. a kind of processing method of useless concentrated phosphoric acid, which is characterized in that it comprises the following steps：
S1. acid is adjusted：Useless phosphoric acid,diluted is added in useless concentrated phosphoric acid to carry out adjusting acid, the concentration for adjusting the waste phosphoric acid after acid is 16~20%,
The mass percentage concentration of the useless concentrated phosphoric acid is 60~70%, and the mass percentage concentration of the useless phosphoric acid,diluted is 5~10%, described useless
Concentrated phosphoric acid and the volume ratio of useless phosphoric acid,diluted are 3~5:1；
S2. thick desulfurization：The waste phosphoric acid after acid will be adjusted to be pumped into thick desulphurization reaction kettle, and add in the thick desulfurization of thick desulfurizing agent progress and obtain
To solidliquid mixture, controlling thick desulphurization reaction material temperature in kettle, the thick desulfurizing agent is CaCO for 50~60 DEG C3, dosage
For synthos precipitation cannot be generated in thick desulphurization reaction kettle；
S3. thick desulfurization press filtration：Solidliquid mixture obtained by step S2 to be sent into thick desulfurization filter press and carries out press filtration, filtrate is spare,
Obtained solid is sulfate precipitation, and the moisture content of the sulfate precipitation is 35~45%；
S4. fine de-sulfur：Filtrate obtained by step S3 is pumped into fine de-sulfur reaction kettle, and adds in desulfurizing agent and obtains secondary solid-liquid mixing
Object, controlling fine de-sulfur material in reactor temperature, the desulfurizing agent is BaCO for 50~60 DEG C3, dosage is obtained by step S3
The 4%~6% of filtrate weight；
S5. fine de-sulfur press filtration：Secondary solidliquid mixture is sent into fine de-sulfur filter press and carries out press filtration, separation of solid and liquid, gained is solid
State is sulfate precipitation, and filtrate is product phosphoric acid；
S6. filter residue mixes：Sulfate precipitation obtained by sulfate precipitation obtained by step S3 and step S5 is mixed, is product sulphur
Hydrochlorate.
A kind of 2. processing method of useless concentrated phosphoric acid as described in claim 1, which is characterized in that thick desulfurization pressure described in step S3
Filter pressure is 0.6~1.0MPa, and filter cloth aperture is 300~350 mesh.
A kind of 3. processing method of useless concentrated phosphoric acid as described in claim 1, which is characterized in that fine de-sulfur pressure described in step S5
Filter pressure is 0.6~1.0MPa, and filter cloth aperture is 300~350 mesh.
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| CN103738933A (en) * | 2013-12-13 | 2014-04-23 | 江苏晓春新材料有限公司 | Method for recovering high purity calcium hydrogen phosphate in sulfur acid-containing waste phosphoric acid |
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| CN103738933A (en) * | 2013-12-13 | 2014-04-23 | 江苏晓春新材料有限公司 | Method for recovering high purity calcium hydrogen phosphate in sulfur acid-containing waste phosphoric acid |
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| Title |
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| 湿法磷酸净化脱硫新工艺;张翠微等;《硫磷设计与粉体工程》;20041231(第6期);第10页1.2，第11页左栏第1段，第12页右栏第2段 * |
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